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Characteristics and Manufacture of Spherical Smokeless Powders

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 doi: 10.5028/jatm.v7i4.466
Characteristics and Manufacture of
Spherical Smokeless Powders
Fernanda Diniz Botelho1, Erick Braga Ferrão Galante1, Álvaro José Boareto Mendes1
ABSTRACT: Smokeless propellants have been studied and
manufactured for many decades. They can exist in various
physical forms and also can have different properties
according to the use of each propellant. One important form
of smokeless powders is the ball powder, which has spherical
grains. The manufacture process of the ball powder has many
advantages over the usual way to manufacture a smokeless
powder. For example, unstable and even deteriorated
nitrocellulose, after being stabilized again, can be used to
produce spherical powders. Also, the process to produce
them requires less water and energy, which can result in
a cheaper way to manufacture powders. In this review, the
spherical powders manufacturing process is described, as
well as the characteristics and advantages of this specific
form of a double-base powder.
KEYWORDS: Double-base propellants, Single-base powders,
Spherical powders, Smokeless powders.
1.Instituto Militar de Engenharia – SE/5 – Seção de Engenharia Química – Rio de Janeiro/RJ – Brazil
Author for correspondence: Erick Braga Ferrão Galante | Instituto Militar de Engenharia – Seção de Engenharia Química | Praça General Tibúrcio, 80 | CEP:
22. 290-270 – Urca – Rio de Janeiro/RJ – Brazil | Email: erickbfgalante@gmail.com
Received: 02/15/2015 | Accepted: 11/02/2015
J. Aerosp. Technol. Manag., São José dos Campos, Vol.7, No 4, pp.398-403, Oct.-Dec., 2015
INTRODUCTION
Smokeless powders are a class of propellants that were
developed in the late 19th century to replace black powder.
There are patents regarding smokeless powder dating back to
the beginning of the 20th century (Piper 1953; Boddicker 1940).
The term “smokeless” refers to the minimal residue left in the
gun barrel following the use of smokeless powder (Heramb
and McCord 2002).
Smokeless propellants can be found in many physical
forms: single or multi-hole cylinders, thin sheets, strips and
others. An important type of smokeless propellants that has
been studied and manufactured for more than 70 years is the
spherical powder, also called ball powder. This variation of
smokeless propellants was first studied by Fredrich Olsen and
peers (Olsen et al. 1936, 1939; Olsen and Tibbitts 1938; Olsen
1942). By the early 1930s, the first patent about the manufacture
spherical powder was published (Valença et al. 2013). It was noticed
that spherical powders had some advantageous characteristics
such as progressive burning rate and high loading density
(U. S. Army 1964), which made it possible to use them in small
ammunition guns.
The history of explosives started with black powder, which
was probably the first explosive to be manufactured. Accidents
involving black powder were reported in 220 BC in a Chinese
document (Akhavan 2004; Valença et al. 2013), when some
alchemists mixed potassium nitrate, sulfur as well as charcoal,
and a big explosion was the result. Black powder was used for
blasting for many years, but the limitations of this explosive became
apparent in the 19th century. For example, mining and tunneling
operations using black powder were very difficult (Akhavan 2004).

A second big event in the history of explosives was the discovery
of sulphuric and nitric acids. With these two substances, it was
possible to nitrate many compounds, making new ones, which
were frequently very unstable and would explode, so they could
eventually replace black powder. In 1861, Alfred Nobel built a
small manufacturing plant to make nitroglycerine, a liquid with
an explosive nature. Nitrocellulose was discovered a few years
after nitroglycerin (Valença et al. 2013), and then scientists around
the world developed many other important explosive substances
such as trinitrotoluene and ammonium nitrate.
The great number of new explosives resulted in the replacement
of black powder as a blasting explosive. However, this compound
is still used in fireworks and in rockets as fuel (Valença et al. 2013).
After the development and manufacture of many explosive
compounds, it became necessary to separate them into groups
in accordance with their properties, for example, their burning
characteristics and stability. A classification by performance
and uses of explosives divides those substances into three
groups: primary explosives, secondary explosives and propellants.
Primary explosives differ from secondary explosives in that they
undergo a very rapid transition from burning to detonation
and can transmit the detonation to less sensitive explosives
(Cooper 1996; Akhavan 2004). Secondary explosives are less
sensitive than primary explosives and do not initiate by heat or
shock. Propellants are combustible materials that do not usually
detonate; they only burn in high velocity (which is defined
as deflagration). The most common way of initiate them is by
using a blasting cap generating heat (Valença et al. 2013; Akhavan
2004; Cooper 1996). Propellants may be named as powders or
gunpowder by some literature. Regarding United Nations risk
classifications, propellants are hazardous goods classified in
general as 1.3C, but depending upon conditions, they can burn
to detonation and are classified as 1.1C (United Nations 2015).
Nitrocellulose and nitroglycerin are energetic bases for
smokeless powders, because they can be used as propellants,
and their burning produces much less residues than that of
black powder (Valença et al. 2013; Heramb and McCord 2002).
All smokeless powders can be placed into one of three different
classes according to the chemical composition of their energetic
ingredients. A single-base powder contains nitrocellulose,
whereas a double-base powder contains nitrocellulose and
nitroglycerine. Nitroguanidine can also be included as a
third energetic base, forming a triple-base propellant (Valença
et al. 2013; Akhavan 2004; Heramb and McCord 2002; Cooper
1996). In some cases, nitroglycerine can be replaced by nitroglycol
J. Aerosp. Technol. Manag., São José dos Campos, Vol.7, No 4, pp.398-403, Oct.-Dec., 2015
Characteristics and Manufacture of Spherical Smokeless Powders
399
because it is more stable at lower temperatures than nitroglycerine
(Valença et al. 2013).
SPHERICAL SMOKELESS POWDERS
CHARACTERISTICS
Spherical smokeless powders were first studied by Fredrich
Olsen and peers (Olsen et al. 1936, 1939; Olsen and Tibbitts
1938; Olsen 1942). Olsen worked for Western Cartridge Company,
an ammunition industry (Hodgdon Powder Co. 2014), and he was
studying new ways to stabilize nitrocellulose because its decom-
position was a problem during World War I. Olsen observed that
a mixture of nitrocellulose, ethyl acetate and water, when agitated,
tended to form small spheres that did not last when the
agitation was interrupted. This fact motivated Olsen to start
studying new ways to manufacture a propellant in a spherical shape.
The spherical powder manufacture process provided many
advantages over common extruded-type powders that were quickly
taken advantage of by ammunition factories. Its key advantages
include: stable long life; high density (ideal for rifle calibers);
adjustable chemistry, which allows the powder to be tailored to
specific cartridge applications through chemistry and geometry;
and lower flame temperature, which allows longer barrel life in
service (Barzanjy 2011; Tao et al. 2010).
The spherical powder is not only substantially spherical in
shape but uniformly dense. It, therefore, has advantages not only
from a ballistic standpoint but also from a loading standpoint.
Spherical grains of the same size and composition burn at the
same rates. That is impossible with angular or oblong grains due
to their varying shapes having different volumes, even though all
may pass through the same screen opening (Olsen et al. 1936).
Another important characteristic that is the progressive
burning rate (Department of the Army 1984; Meyer et al. 2007;
Valença et al. 2013). This is possible because, while a powder
grain burns from the outside towards the inside, it reaches
different layers with higher burning rates, as well as higher
temperatures. The modifying agents and surface coats burn
first, and then the inner part of the grain, made of nitrocellulose
(which has a higher burning heat), is reached. A progressive
burning is advantageous because it makes possible to keep
the pressure inside the barrel high for a longer time, and a
higher pressure peak is avoided. In general, the behavior of the
burning allows the formation of a plateau at a high pressure,
which gives the same overall energy under the curve if there
was a single higher pressure peak. This is advantageous because
 Botelho FD, Galante EBF, Mendes AJB
400
the gun barrel will not have to tolerate very big pressures
(U. S. Army 1964).
In small arms ammunition, particularly where progressive
burning powder is used as the propellant, it often happens
that the propellant charge does not completely burn inside the
barrel and that combustion thereof is prolonged even after
the projectile or shot charge has left the barrel. This prolonged
combustion is objectionable because the burning particles
of powder are expelled from the barrel of the arm behind
the projectile, and the energy which would otherwise be
imparted to the projectile is lost. In accordance with Olsen’s
invention (Olsen and Tibbitts 1938), the spherical powder
charge is also clean burning and is completely consumed by
combustion by the time the projectile or shot charge leaves
the barrel whereby the objectionable conditions, such as
deposits in the barrel and the ejection of luminous particles of
powder from the muzzle of the gun, are substantially reduced.
PRODUCTION
Spherical smokeless powder is generally made from
nitrocellulose as the base material. The nitrocellulose may be derived
from purified cellulose, such as from cotton linters or wood,
which is then nitrated by being treated with nitric and sulfuric acids
(Olsen 1942; Valença et al. 2013; Department of the Army 1984).
In the manufacture of nitrocellulose, it is necessary to subject
the nitrated cellulose to extensive purification treatments in
order to remove the residual acid and unstable esters from the
nitrocellulose fibers. A large amount of water is required for these
purification treatments, and a considerable consumption of heat
is necessary (Olsen 1942). In order to convert nitrocellulose,
which has been purified, into gelatinized or colloided smokeless
powder grains, it is customary to replace the water contained
in the nitrocellulose with alcohol by means of a displacement
process (Olsen et al. 1936).
Nitrocellulose which has deteriorated or contained centers
of high acid concentration, as is frequently present in aged
cannon powder, may be purified and stabilized to an extent
sufficient to for use as propellant. This may be rendered suitable
by grinding the deteriorated nitrocellulose powder in water
slurry and thereafter agitating the slurry in a sufficient quantity
of a solvent, such as water, to wash out and disperse the centers
of high acidity. It is also desirable to add to the slurry a sufficient
quantity of a neutralizing agent, such as calcium carbonate or
other mild alkali, so as to neutralize the acid which may be washed
out of the nitrocellulose spheres/pieces (Olsen et al. 1939, 1940).
J. Aerosp. Technol. Manag., São José dos Campos, Vol.7, No 4, pp.398-403, Oct.-Dec., 2015
Regarding the production of the smokeless powder, Olsen
and his co-workers developed a process to manufacture a
smokeless powder in a manner so as to secure a superior
product irrespective (within limits) of the base. The base
may be nitrocellulose, and its kind and character, as well as
composition, may be varied; it may be wholly or partially
purified fibrous nitrocellulose; it may be dense colloided
nitrocellulose in the form of existing powder, or of good, poor
or indifferent stability (Silk 1945; Olsen et al. 1936). Also,
during the course of operations, the product is purified and
stabilized, and the incorporation of additional ingredients,
such as stabilizers and modifying agents (burning regulators
or accelerators), are added (Olsen et al. 1936).
In accordance with Olsen’s invention (Olsen et al. 1936),
a greatly simplified procedure can be used for accomplishing
the desired purification of the nitrocellulose as well as the
gelatinization thereof and the formation of grains. If the
nitrocellulose is impure and in an unstable condition, it is
treated with a suitable solvent to form a lacquer from which the
impurities are then removed by agitation in a suitable non-solvent
bath, such as water. By distilling off a sufficient amount of the
solvent during continued agitation, the gelatinized nitrocellulose
becomes converted to preliminary grains. If the solvent for
the powder base is selected so that it will be substantially
immiscible with the non-solvent bath, and conditions tending
to produce an emulsion with the powder base in the solution as
the internal phase are maintained, the preliminary grains may be
resolved into globular form and may, if desired, be completely
solidified and employed as a propellant powder in this shape,
without further operations of grain formation (Olsen 1942).
To protect the resulting powder against autocatalytic
decomposition, one of the usual stabilizers as, for example,
the centralities or diphenylamine, may be added to the lacquer
so that the desired amount becomes incorporated within the
individual particles of lacquer (Olsen 1942). The stabilizer is not
only uniformly distributed throughout the globules formed within
the medium and the grains thereafter formed from globules, but
any acidic or deteriorated elements present will be distributed
throughout the vehicle or medium (Olsen et al. 1936). The
modifying agents such as deterrents or accelerators may also
be incorporated with a grain and distributed throughout the
grain in a manner similar to that of incorporating the stabilizer.
In general, the desired formation of the grains is accomplished
by dispersing globules of the base (such as nitrocellulose) in
a medium. This is accomplished by subjecting the base and a

solvent to agitation in a non-solvent medium (such as water) so
as to produce globules that are individually consolidated in order
to form grains which are spherical (Carlucci and Jacobson 2008;
Olsen et al. 1936; U. S. Army 1964). A volatile solvent may also
be used to produce globules, being before vaporized by heating
(Olsen et al. 1936). Suitable solvents include ethyl acetate, isopropyl
acetate, methyl isobutyl ketone, as well as other organic liquids
which are solvents for nitrocellulose not completely miscible with
water (Coffee 1964; Silk 1945), and are sufficiently volatile so that
they may be vaporized without having to resort to temperatures
which are unsafe or inconvenient. The treatment with the solvent
is preferably carried out to an extent sufficient to convert all of
the nitrocellulose present in a lacquer (Olsen 1942).
The desired amount of solvent may be added to the slurry of
nitrocellulose dust in the form of a spray and, in this manner, small
globules of the solvent may be readily distributed throughout
the mixture. During agitation and heating, the surfaces of the
particles of nitrocellulose dust become softened due to the
gelatinizing action of the solvent and tend to coalesce, forming
clusters comprising a number of dust particles. This action
may be explained since all liquid or plastic two-phase systems
tend to a condition of minimum surface energy which can be
accomplished by coalescence (Olsen et al. 1936, 1940).
The production of globules or the production of the
quasi-emulsion may be secured in various ways. In accordance
with Olsen’s invention (Olsen et al. 1936), the base is dissolved
in a solvent and the colloidal solution or lacquer is agitated
rather violently in a non-solvent vehicle in the presence of the
protective colloid and a neutralizer to form the globules. The
protective colloid performs the function of effecting a quasi-
emulsion between the base and solvent and the non-solvent
medium, with the base and solvent as the internal phase. The
base is agitated with a solvent distributed in the non-solvent
vehicle so as to form an emulsion with the medium as the internal
phase; upon the addition of the protective colloid the emulsion
is broken and under agitation inverted with the medium as the
external phase. The neutralizer is added to remove the high-
acidity centers. A suitable neutralizer is calcium carbonate in
the form of purified prepared chalk (Olsen et al. 1936, 1939).
The globules, which are distributed throughout the medium,
are then subjected to treatment to extract the solvent, through
distillation of the solvent secured by heating the medium to near
the vaporizing point of the solvent. The distillation is so carried
out as to effect a gradual vaporization of the solvent from the
several globules; the process is preferably carried out by effecting
J. Aerosp. Technol. Manag., São José dos Campos, Vol.7, No 4, pp.398-403, Oct.-Dec., 2015
Characteristics and Manufacture of Spherical Smokeless Powders
401
vaporization at a rate decreasing from the beginning to the end of
the vaporization period and at a rate less than the rate of diffusion
of the solvent from the interiors to the exteriors of the globules.
Such a distillation secures a solid grain as distinguished from
one which is hollow and porous (Olsen et al. 1936).
After formation of the globules in the medium or vehicle,
and after distillation of the solvent from the several globules to
form grains, the medium is permitted to cool to a temperature
sufficiently low to permit any modifying agent or stabilizer
dissolved in the normally non-solvent medium to separate
out at the lower temperature. In the case of the modifying
agent, such as deterrent, it will become deposited on the grains
so as to provide a surface treatment in the form of a coating
or impregnation (Olsen et al. 1936). Figure 1 represents a
manufacture process of spherical grains of smokeless powders.
The finishing operations are similar to the ones that are usually
carried out during the manufacture of a single-base smokeless
powder. After cooling of the medium, and when the grains have
become consolidated or hardened, they may be subjected to a
screening operation, in which the oversizes can be sent back for
reworking and the screened grains can be subjected to a wringing
operation and thereafter to a drying operation. The grains may
be surface treated prior to drying with a suitable modifying
Nitrocellulose
Deterrent Solvent
Solvent Colloid
Stabilizer Neutralizer
Aqueous solution
Lacquer
(water)
Agitate
Reactor Distill
Cool
Finishing operations
Based upon the work of Olsen et al. (1936).
Figure 1. Spherical powder manufacturing process.
 Botelho FD, Galante EBF, Mendes AJB
402

agent, such as a deterrent or an accelerator. The coating may
comprise nitroglycerin which acts as an accelerator; in that it
allows the powder to be more readily ignitable and also acts as
a waterproofing agent, rendering the powder non-hygroscopic.
A suitable deterrent such as dibutylphthalate may be used along
with the nitroglycerin or other accelerator and waterproofing
agent. The grains may be then dried and glazed in the usual
manner and thereafter blended if desired (Olsen et al. 1936, 1940).
The size of the grains is a function of the extent and the violence
of the agitation as well as the amount of protective colloid and the
viscosity of the dissolved base (Olsen et al. 1936; Valença et al.
2013). The grain size decreases with the increase of rotor speed,
the increase of percentage of the colloid and the viscosity of the
nitrocellulose. Furthermore the amount of solvent employed
affects not only the size, shape and surface of the resultant grains,
but also the gravimetric density thereof (Schaefer 1939; Olsen et
al. 1940). Small amounts of solvent give a small rough cluster of
particles as the grains while larger amounts of solvent give more
spherical smoother grains. The rate at which the temperature is
raised during evaporation of the solvent affects both the granulation
carried out using Fig. 2, which shows the difference between the
thrust produced by propellants with different burning characteristics.
Progressive burning occurs when the thrust produced increases
with time and with distance traveled, inside the barrel (Kosanke
2012). During a regressive burning, the surface area decreases
with time, and so does the thrust. The neutral burning happens
when the burning area is approximately constant, which results
in a constant thrust over the burning period. The pressure peak
is higher and is reached first in a regressive burning rate because,
as the burning area decreases, the gas production lowers, so the
maximum pressure occurs in the very beginning of the barrel. On
the other side, if a progressive burning propellant is used, the peak
pressure is limited to a value that may be tolerated by the gun
(Moss et al. 1983; U. S. Army 1964). It is also important to address
the effect of adding high explosives in the composition on the
propellant performance (Zhu et al. 2012).
Table 1. Comparison between spherical powders and
common powders.
Powder Advantages Disadvantages

and density of the resultant powder (Schaefer 1939). Unstable nitrocellulose can
The process for the manufacture of spherical powder, which be used. The plant to
Deteriorated nitrocellulose produce cannot be
Olsen and his co-workers have devised, combines nicely with from cannon powders can be used to produce
Olsen’s process for the quick stabilization of nitrocellulose to form a Spherical reused. other types of
powder Loading spherical grains is powders.
sequence of operations by which a finished powder may be produced easier. Can only be used
more rapidly and more safely than by the usual process. It supplies The grain formation is carried in small caliber
in only one reactor. ammunitions.
a convenient means of making up a powder which contains non- Progressive burning rate.
volatile solvents throughout the mass of the grains or deterrent or Many physical forms can be High consumption
accelerant coatings upon their surface (Urbanski 1967). Other
produced. of water and
It can be used in bigger energy during the
Although the spherical powder starts as pure nitrocellulose, double-base
ammunition calibers. production process.
powders
the finished product is a double-base propellant, since The same plant can be used to Stable nitrocellulose
produce different powders. is necessary.
nitroglycerin is added after shaping and its content is created
by surface impregnation.

Pressure
COMPARISON
Pressure Neutral burning
Table 1 provides a comparison between spherical powders limit of gun
Regressive burning
and other common double-base smokeless powders with
Progressive burning
respect to manufacture process, characteristics and uses.
It aims to briefly compare spherical powders against other
double-base propellants. This is important since their production Shot start
pressure
is more complex (hence expensive) than that of extruded
propellants. Due to this, they are used mainly when the Shot start position Muzzle Time

ammuntion does so requires.

Based upon the work of Moss et al. (1983).
Another important comparison aspect between propellants is
the effectiveness and burning characteristics. This comparison is Figure 2. Pressure-time curves for different burning rates.

J. Aerosp. Technol. Manag., São José dos Campos, Vol.7, No 4, pp.398-403, Oct.-Dec., 2015

In Fig. 2, “Shot start position” and “Muzzle” correspond to the time
when these positions are reached. The curves shown in Fig. 2 can be
determined using a closed vessel. The spherical powder can be used
in small ammunitions to provide a greater muzzle velocity, which
will result in a bigger kinetic energy being transferred to the target.
A typical peak pressure for a 5.56-mm ammunition is
354 MPa (Moss et al. 1983); it is considered when designing
a new gun or barrel, hence this is the value considered to be
compared against.
CONCLUSION
The great advantage of the spherical powder manufacture
process is the possibility of using deteriorated and unstable
nitrocellulose. Aged powders that would be destroyed can
be reused, which results in a lower production cost. Also, the
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Characteristics and Manufacture of Spherical Smokeless Powders
403
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